WO2017022812A1 - Capteur de gaz électrolytique à potentiel constant - Google Patents

Capteur de gaz électrolytique à potentiel constant Download PDF

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Publication number
WO2017022812A1
WO2017022812A1 PCT/JP2016/072872 JP2016072872W WO2017022812A1 WO 2017022812 A1 WO2017022812 A1 WO 2017022812A1 JP 2016072872 W JP2016072872 W JP 2016072872W WO 2017022812 A1 WO2017022812 A1 WO 2017022812A1
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WO
WIPO (PCT)
Prior art keywords
gas
electrode
constant potential
gas sensor
electrolytic
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PCT/JP2016/072872
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English (en)
Japanese (ja)
Inventor
近藤克典
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新コスモス電機株式会社
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Publication date
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Priority to CN201680045156.9A priority Critical patent/CN107850563A/zh
Publication of WO2017022812A1 publication Critical patent/WO2017022812A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/404—Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid, e.g. Clark-type oxygen sensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems

Definitions

  • a reaction electrode for electrochemically reacting a gas to be detected as a gas electrode for detecting gas, a counter electrode with respect to the reaction electrode, and a reference electrode for controlling the potential of the reaction electrode are brought into contact with an electrolytic solution accommodated in an electrolytic cell.
  • the present invention relates to a constant potential electrolysis gas sensor.
  • a conventional constant potential electrolytic gas sensor is configured such that an electrode is provided facing an electrolytic solution storage part of an electrolytic cell in which an electrolytic solution is densely stored. For example, an electrode is detected as a gas electrode that detects gas.
  • an electrode is detected as a gas electrode that detects gas.
  • a potentiostat circuit for setting the potential is connected.
  • a gas-permeable porous PTFE film having water repellency is coated with a noble metal catalyst such as platinum, gold, palladium, etc.
  • an electrolyte an acidic aqueous solution such as sulfuric acid or phosphoric acid is used. Was used.
  • the constant potential electrolytic gas sensor generates a current corresponding to the change in the surrounding environment between the reaction electrode and the counter electrode by controlling the potential of the reaction electrode to be constant with respect to the change in the surrounding environment. . Then, by utilizing the fact that the potential of the reaction electrode does not change and the oxidation-reduction potential varies depending on the gas type, it becomes possible to selectively detect the gas depending on the set potential of the potentiostat circuit. Further, by changing the catalyst used for the gas electrode, it is possible to have high selectivity for the target gas.
  • constant potential electrolytic gas sensor which is a conventional technique in the present invention, is a general technique, and thus does not show conventional technical documents such as patent documents.
  • the air layer may expand and bubbles may enter the sensor through a through hole formed on the gas ventilation part side.
  • the contact area wetting area
  • the contact area wetting area
  • an object of the present invention is to provide a constant potential electrolytic gas sensor that can suppress the formation of bubbles at least on the surface of the counter electrode.
  • a constant potential electrolytic gas sensor controls a reaction electrode for electrochemically reacting a gas to be detected as a gas electrode for detecting gas, a counter electrode for the reaction electrode, and a potential of the reaction electrode.
  • a constant potential electrolytic gas sensor provided with a reference electrode in contact with an electrolyte contained in an electrolytic cell, the first characteristic configuration of which is a bubble that suppresses the formation of bubbles at least on the surface of the counter electrode It is in the point provided with formation suppression means.
  • the bubble formation suppressing means even when the temperature of the sensor changes suddenly due to the influence of the disturbance, for example, it is difficult for bubbles to be mixed from a through hole formed on the counter electrode side.
  • the bubbles mixed on the surface of the counter electrode are difficult to reach. Accordingly, it is possible to suppress the formation of bubbles at least on the surface of the counter electrode, and thus it is possible to suppress a sudden change in the indicated value of the sensor.
  • the second characteristic configuration of the constant potential electrolytic gas sensor according to the present invention is that the bubble formation suppressing means is a water retaining member that absorbs and holds the electrolytic solution.
  • the bubble formation suppressing means is a water retaining member, it is more difficult for bubbles mixed in at least the surface of the counter electrode facing the electrolyte container to reach, and it is ensured that bubbles are formed on the surface of the counter electrode. Can be suppressed.
  • a third characteristic configuration of the constant potential electrolytic gas sensor according to the present invention is that an oxygen permeable membrane that transmits oxygen is disposed in a gas ventilation portion that discharges gas formed on the counter electrode and the reference electrode. .
  • the fourth characteristic configuration of the potentiostatic gas sensor according to the present invention is that the filling rate of the water retaining member is 90% or more.
  • each gas electrode since the surface of each gas electrode can be reliably covered, it is difficult for the mixed bubbles to reach the surface of each gas electrode, and it is ensured that bubbles are formed on the surface of each gas electrode. Can be suppressed.
  • bubbles generated due to electrode reactions or the like in each gas electrode, or air dissolved in the electrolyte solution due to a rapid temperature change, or by intrusion of air in a sudden pressurization state It can be avoided that the surface of each gas electrode is covered with air, the reaction area of each gas electrode is reduced, and the indication becomes unstable.
  • a fifth characteristic configuration of the constant potential electrolytic gas sensor according to the present invention is that the water retention member has a bulk density of 0.05 to 0.30 g / cm 3 .
  • the water retention member when the water retention member is disposed in the electrolyte container, the water retention member can be disposed so as to press each gas electrode to some extent, so that the contact state between the water retention member and each gas electrode is ensured. Can be secured. Thereby, at least the bubbles mixed on the surface of the counter electrode are more difficult to reach.
  • the constant potential electrolytic gas sensor X controls a reaction electrode 11 that causes a gas to be detected to electrochemically react as a gas electrode 10 that detects gas, a counter electrode 12 with respect to the reaction electrode 11, and a potential of the reaction electrode 11.
  • the reference electrode 13 is provided so as to be in contact with the electrolytic solution 20 accommodated in the electrolytic cell 30.
  • This constant potential electrolytic gas sensor X includes a bubble formation suppressing means 50 that suppresses the formation of bubbles on at least the surface of the counter electrode 12.
  • the reaction electrode 11, the counter electrode 12, and the reference electrode 13 are formed by applying and baking a paste made of a known electrode material on the surface of a porous gas permeable film 14 having water repellency.
  • the gas permeable membrane 14 may be any membrane as long as it is hydrophobic and has a property of transmitting gas.
  • a porous PTFE (polytetrafluoroethylene) membrane having chemical resistance may be used. it can.
  • the reaction electrode 11, the counter electrode 12, and the reference electrode 13 are composed of a gas diffusion electrode including a catalyst and a hydrophobic resin (gas permeable membrane 14).
  • a catalyst platinum (Pt), gold (Au), ruthenium (Ru), Ruthenium oxide (RuO2), palladium (Pd), platinum-supported carbon (Pt / C), etc. are preferably used.
  • the counter electrode 12 and the reference electrode 13 of the present embodiment have a mode in which the counter electrode 12 is formed in the upper half and the reference electrode 13 is formed in the lower half in one gas permeable membrane 14, but is limited to such a mode. It is not something. Between the counter electrode 12 and the reference electrode 13, the slit 14a in which an electrode is not formed is formed.
  • the reaction electrode 11 and the reference electrode 13 are arranged to face each other, and the counter electrode 12 and the reference electrode 13 are arranged on the gas ventilation part 33 side.
  • a space between the reaction electrode 11, the counter electrode 12, and the reference electrode 13 serves as an electrolyte solution storage unit 31 that stores the electrolyte solution 20.
  • the electrolytic solution 20 may be an acidic aqueous solution such as sulfuric acid or phosphoric acid, but is not limited thereto.
  • the gas to be detected is introduced into the sensor from the gas introduction part 32 and reacts on the reaction electrode 11.
  • the buffer filter 35 is a buffer film that prevents deformation of each electrode and prevents leakage of the electrolyte solution 20.
  • a porous Teflon (registered trademark) film having a porosity of about 80% can be used. It is not limited to.
  • Each gas electrode 10, gas permeable membrane 14, buffer filter 35, and O-ring 15a are fixed by a lid member 16 (16A, 16B) of the electrolytic cell 30.
  • An internal pressure adjusting hole 17 having a small diameter of about 0.5 to 2 mm is formed at one end of the electrolytic cell 30.
  • a porous sheet 18 is disposed on the internal pressure adjusting hole 17 on the side of the electrolytic solution containing portion 31.
  • the electrolyte storage unit 31 has two large-diameter storage units 31b through a small-diameter channel 31a. When the flow path 31a has a small diameter of about 2 to 4 mm, the electrolytic solution 20 is unlikely to flow backward from one housing portion 31b to the other housing portion 31b due to the surface tension of the electrolytic solution 20.
  • the electrolytic cell 30 and the lid member 16 constituting the housing may be made of a synthetic resin having corrosion resistance, for example, a metal such as hard vinyl chloride or nickel alloy.
  • Through holes 16a and 16b are respectively formed in the lid member 16A formed on the gas introduction part 32 side and the lid member 16B formed on the gas ventilation part 33 side, and gas is introduced through the through hole 16a.
  • the gas is discharged and introduced through the through hole 16b. Since the position where the through hole 16b is formed corresponds to the position of the slit 14a where no electrode is formed, gas can be discharged or introduced through the slit 14a and the through hole 16b.
  • the gas layer 33 that discharges the gas formed on the side of the counter electrode 12 and the reference electrode 13 is provided with an air layer 40 and an oxygen permeable membrane 41 that transmits oxygen.
  • the oxygen permeable membrane 41 is not particularly limited as long as it has oxygen permeation performance.
  • FEP tetrafluoroethylene hexafluoropropylene copolymer resin
  • PFA perfluoroalkyl vinyl ether copolymer
  • the oxygen permeable film 41 By disposing the oxygen permeable film 41 as in this configuration, it is possible to prevent the surrounding interference gas (other than oxygen) from entering the counter electrode 12 and the reference electrode 13 from the gas ventilation portion 33.
  • the constant potential electrolytic gas sensor X of the present invention includes bubble formation suppressing means 50 that suppresses the formation of bubbles on at least the surface of the counter electrode 12.
  • the bubble formation suppressing means 50 may be configured to suppress the formation of bubbles on the surface of the other gas electrode 10 (reaction electrode 11 and reference electrode 13) in addition to the counter electrode 12.
  • the air layer 40 may expand greatly and air bubbles may be mixed in through the through holes 16b formed on the gas ventilation part 33 side. If the mixed bubbles reach the surface of the electrode and, for example, bubbles are formed on the surface of the counter electrode 12, the contact area between the electrolytic solution 20 and the counter electrode 12 may decrease, and the indicated value of the sensor may suddenly increase. .
  • the bubble formation suppressing means 50 of the present invention it is difficult for air bubbles to be mixed from the through hole 16b even when the temperature of the sensor is suddenly changed due to the influence of disturbance, and the bubble is prevented from passing through the through hole 16b.
  • the bubble formation suppressing means 50 is the water retaining member 37, it is more difficult for bubbles mixed in at least the surface of the counter electrode 12 facing the electrolyte container 31 to reach, and it is ensured that bubbles are formed on the surface of the counter electrode 12. Can be suppressed.
  • the water retaining member 37 may be disposed so as to suppress at least the formation of bubbles on the surface of the counter electrode 12, and preferably suppresses the formation of bubbles on the surfaces of the reaction electrode 11 and the reference electrode 13. What is necessary is just to arrange
  • the water retaining member 37 can be filled in the entire surface (100%) of one accommodating portion 31b (the side where the gas electrode 10 is disposed) in the electrolyte accommodating portion 31 as in the present embodiment.
  • the present invention is not limited to such an embodiment, and the water retaining member 37 is filled with, for example, 90% or more, specifically about 90 to 95% of one accommodating portion 31b (side on which the gas electrode 10 is disposed). What is necessary is just to fill so that it may become a rate.
  • the surface of each gas electrode 10 can be reliably covered, so that the mixed bubbles are less likely to reach the surface of each gas electrode 10. It is possible to reliably suppress the formation of bubbles on the surface.
  • the water retaining member 37 is an aspect that absorbs and holds the electrolytic solution 20, the water retaining member 37 has a space in which the electrolytic solution 20 can be retained. Therefore, even if it is a case where the water retention member 37 is filled in the whole surface of the accommodating part 31b, the contact state of each gas electrode 10 and the electrolyte solution 20 can be maintained favorable.
  • the water retaining member 37 is not particularly limited as long as it is a water absorbing member capable of holding the electrolytic solution 20 such as a water retaining fiber (for example, glass fiber, ceramic fiber, etc.) or a water absorbing polymer.
  • the bulk density of the water retaining member 37 is preferably 0.05 to 0.30 g / cm 3 .
  • MGP manufactured by Nippon Sheet Glass Co., Ltd.
  • the density is about 0.18 g / cm 3 and the space ratio is about 90%
  • MC paper manufactured by Nippon Sheet Glass Co., Ltd.
  • the bulk density of the water retaining member 37 is 0.08 g.
  • OR-125 manufactured by Asahi Textile Industry Co., Ltd.
  • the bulk density of the water retaining member 37 and the actual product are not limited to these.
  • a plurality of such water retaining members 37 may be arranged in the electrolyte solution storage unit 31 in a stacked manner.
  • the water retaining member 37 With the structure of the water retaining member 37 described above, the water retaining member 37 can be pushed to some extent to fill the accommodating portion 31b, and the water retaining member 37 can be disposed so as to press each gas electrode 10 to some extent. And the contact state between the gas electrodes 10 can be reliably ensured. As a result, at least air bubbles mixed on the surface of the counter electrode 12 are more difficult to reach.
  • Such a constant potential electrolytic gas sensor X includes a current measuring unit capable of detecting a current based on electrons generated on the reaction electrode 11 due to a reaction of the gas to be detected, and a potential control unit capable of controlling the potential of the reaction electrode 11. It is used as a gas detection device by connecting to a gas detection circuit (not shown).
  • the constant potential electrolytic gas sensor X of the present invention is used for detecting oxygen gas, hydride gas such as silane, phosphine, germane, arsine and diborane, and detecting toxic gas such as carbon monoxide and hydrogen sulfide.
  • the filter means 60 for filtering the interference gas is provided on the lid member 16A on the gas introduction part 32 side.
  • the filter means 60 is disposed on a frame 16c formed on the lid member 16A.
  • the filter means 60 has a structure in which a plurality of filter layers 61 including activated carbon and silica gel for filtering interference gas are accommodated in a cylindrical container 60a, and both sides of the filter layers 61 are holding members such as meshes.
  • the present invention is not limited to such a mode.
  • cylindrical member 34 examples include ceramics such as alumina and zirconia, but are not limited thereto.
  • the long dimension of the cylindrical member is 2.0 mm or more, preferably 2.0 to 6.0 mm.
  • the diameter of the pinhole 34a is preferably about 0.05 mm.
  • the gas ventilation part 33 side may be sealed with a sealing means 36 such as an adhesive or packing in order to ensure airtightness other than the pinhole 34a.
  • the gas flow on the gas ventilation part 33 side can be limited to the pinhole 34a.
  • the through hole 16b on the gas ventilation portion 33 side small and long, interference gas or the like is less likely to be mixed into the inside of the sensor (electrolyte accommodating portion 31 or the like).
  • the cylindrical member 34 in which the pinhole 34a is formed can be used as the air bubble formation suppressing means 50.
  • the water retaining member 37 in the above-described embodiment may be provided, or even if not provided, at least the surface of the counter electrode 12 by the cylindrical member 34. It is possible to suppress the formation of bubbles on the surface, and thus it is possible to suppress a sudden change in the indicated value of the sensor.
  • the shape of the cylindrical member 34 is preferably a cylindrical shape, but is not limited to this, and may be a prismatic shape or the like.
  • the pin member 34a provided in the cylindrical member 34 may be one or plural.
  • the number of pinholes 34a is not particularly limited. In the present embodiment, a case where one pinhole 34a is formed in each cylindrical member 34 will be described.
  • the amount of gas introduced can be adjusted by the number of pinholes 34a. Even if condensation occurs in the gas introduction part 32, if a plurality of pinholes 34a are formed, all the pinholes 34a are not easily blocked by condensation, and gas discharge or introduction due to gas reaction is hindered. Can be prevented in advance. Since the amount of gas introduced can be adjusted not only by the number of pinholes but also by the length and diameter of the pinholes, it may be set appropriately according to the interference gas to be suppressed.
  • the constant potential electrolytic gas sensor X of the present example was set as the following mode. That is, in the controlled potential electrolytic gas sensor X of the embodiment of FIG. 1, the buffer filter 35 having a thickness of 1 mm is a porous Teflon (registered trademark) membrane (PTFE membrane), the water retaining member 37 is a glass fiber member, and oxygen permeation is performed.
  • the membrane 41 was made of tetrafluoroethylene hexafluoropropylene copolymer resin (FEP), the filter layer 61 was made of four activated carbon layers, and the holding member 62 was made of SUS mesh. Further, the diameters of the through holes 16a and 16b were 2 mm, and the width of the slit 14a formed between the counter electrode 12 and the reference electrode 13 was 1.5 mm.
  • the constant potential electrolytic gas sensor X of the present embodiment is configured such that the water retaining member 37 and the oxygen permeable membrane 41 are not used, and the cylindrical member 34 in which the pinhole 34a is formed is disposed.
  • the long dimension of the said cylindrical member 34 was 3.0 mm, and the diameter of the pinhole 34a was 0.05 mm.
  • the sensor which does not provide a pinhole was used as a constant potential electrolysis type gas sensor of a comparative example. That is, the diameter of the through hole 16b on the gas ventilation part 33 side in this sensor was 2.0 mm, and the long dimension was 2.0 mm.
  • the controlled potential electrolytic gas sensor X of the present invention As a result, in the controlled potential electrolytic gas sensor X of the present invention (FIG. 5), the sensor indicated no significant fluctuations and was considered stable. Therefore, it was confirmed that the constant potential electrolysis gas sensor X of the present invention has the same performance as the case where the oxygen permeable membrane is used even if interference gas exists in the surroundings.
  • the indicated value of the sensor fluctuated greatly, and the sensor output was considered to be unstable.
  • the diameter of the through hole 16b is larger than the pinhole 34a of the constant potential electrolytic gas sensor X of the present invention. It was confirmed that gas could easily enter and the instructions were not stable.
  • a reaction electrode for electrochemically reacting a gas to be detected as a gas electrode for detecting gas, a counter electrode with respect to the reaction electrode, and a reference electrode for controlling the potential of the reaction electrode are brought into contact with an electrolytic solution accommodated in an electrolytic cell. It can utilize for the constant potential electrolytic gas sensor provided.

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Abstract

La présente invention concerne un capteur de gaz électrolytique à potentiel constant X comprenant comme électrodes de gaz qui détectent du gaz, une électrode de réaction 11 qui soumet un gaz à détecter à une réaction électrochimique, une contre-électrode 12 faisant face à l'électrode de réaction 11, et une électrode de référence 13 qui commande le potentiel de l'électrode de réaction 11 d'une manière établissant un contact avec une solution d'électrolyte 20 dans un bain électrolytique 30, le capteur de gaz électrolytique à potentiel constant comprenant un moyen d'inhibition de formation de bulles d'air 50 qui inhibe la formation de bulles d'air sur la surface d'au moins la contre-électrode 12.
PCT/JP2016/072872 2015-08-03 2016-08-03 Capteur de gaz électrolytique à potentiel constant WO2017022812A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201680045156.9A CN107850563A (zh) 2015-08-03 2016-08-03 恒电位电解式气体传感器

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JP2015-153282 2015-08-03
JP2015153282A JP6752558B2 (ja) 2015-08-03 2015-08-03 定電位電解式ガスセンサ

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WO2017022812A1 true WO2017022812A1 (fr) 2017-02-09

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Publication number Priority date Publication date Assignee Title
JP6517423B1 (ja) * 2018-12-27 2019-05-22 新コスモス電機株式会社 定電位電解式ガスセンサ
JP6517422B1 (ja) * 2018-12-27 2019-05-22 新コスモス電機株式会社 定電位電解式ガスセンサおよび定電位電解式ガスセンサを備える吸引式ガス検知器

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6140557A (ja) * 1984-07-31 1986-02-26 Japan Storage Battery Co Ltd ガルバニ電池式酸素センサ−
JPH03125959A (ja) * 1989-10-11 1991-05-29 New Cosmos Electric Corp 電解式ガスセンサ
JPH06242059A (ja) * 1993-02-19 1994-09-02 Gastec:Kk 電気化学式ガスセンサ

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GB8430803D0 (en) * 1984-12-06 1985-01-16 Bergman I Electrochemical cell
JP4507235B2 (ja) * 2003-10-30 2010-07-21 理研計器株式会社 電気化学式ガスセンサ
CN101275923B (zh) * 2007-03-26 2013-04-10 华瑞科学仪器(上海)有限公司 气体传感器
JP6212768B2 (ja) * 2013-03-30 2017-10-18 新コスモス電機株式会社 電気化学式ガスセンサ
JP6315983B2 (ja) * 2013-12-26 2018-04-25 新コスモス電機株式会社 定電位電解式ガスセンサ
CN204142678U (zh) * 2014-10-24 2015-02-04 荆州市爱尔瑞科技有限公司 一种三电极电化学气体传感器

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6140557A (ja) * 1984-07-31 1986-02-26 Japan Storage Battery Co Ltd ガルバニ電池式酸素センサ−
JPH03125959A (ja) * 1989-10-11 1991-05-29 New Cosmos Electric Corp 電解式ガスセンサ
JPH06242059A (ja) * 1993-02-19 1994-09-02 Gastec:Kk 電気化学式ガスセンサ

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JP6752558B2 (ja) 2020-09-09
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